CN1039321A - The method of electrolytic reduction-extraction neptunium recovery from radioactive liquid waste - Google Patents
The method of electrolytic reduction-extraction neptunium recovery from radioactive liquid waste Download PDFInfo
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- CN1039321A CN1039321A CN 88104195 CN88104195A CN1039321A CN 1039321 A CN1039321 A CN 1039321A CN 88104195 CN88104195 CN 88104195 CN 88104195 A CN88104195 A CN 88104195A CN 1039321 A CN1039321 A CN 1039321A
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Abstract
The present invention is a kind of method that adopts electrolytic reduction-extraction neptunium recovery from radioactive liquid waste, in simple reduction cell with radioactive liquid waste in pentavalent neptunium be reduced into tetravalence, use phosphorus extractant quantified extract neptunium recovery again.The present invention is applicable to removal and neptunium recovery and other actinide from the high activity liquid waste of spentnuclear fuel aftertreatment.
Description
The electrolytic reduction and the recovery method of neptunium in the strong radioactive waste liquid that the present invention relates to obtain in the aftertreatment of reactor spentnuclear fuel, and the removal and the recovery of actinide in the strong radioactive waste liquid.
Contain actinides such as trace uranium, plutonium, curium, neptunium in the high activity liquid waste that produces in the reactor spentnuclear fuel last handling process, the long-life alpha nucleic in them comprises
237Np is the main nucleic of decision radioactive waste long-term hazards.In order to reduce the long-term hazards of nuclear waste, will from high activity liquid waste, remove these actinides.These actinides of separating can return again does fuel or conversion in the reactor, both can be transformed into short half life nucleic, can save nuclear fuel again.
The chemical form of neptunium in solution is very complicated, because the disproportionation reaction of neptunium in the aqueous solution, the redox reaction that irradiation effect and photochemical reaction cause makes neptunium exist simultaneously with multiple valence state in aqueous solution, wherein pentavalent neptunium (N
PO
2 +) extracting power very weak, usually not by phosphorus extractant such as tributyl phosphate extractions such as (TBP).Therefore in the recovery extraction process of neptunium, must regulate the valence state of neptunium.Usually readjust prices with the method that adds reductant-oxidant.BE-749108 Ce
(IV), V
(V)And Cr
(VI)Deng N
P (V)Be oxidized to N
P (VI), extract neptunium with the TBP extraction again.DT-2048527 0.05mol/l N
2H
4With 0.005mol/l Fe(SO
3NH
2) 2 N
P (V)Be reduced into tetravalence, from sulfuric acid medium, extract neptunium recovery with three lauric acid amine.US3,595,629 usefulness, 0.025～0.05mol/l hydrazine is made reductive agent, and neptunium is reduced into tetravalence, with dibutyl butyl phosphine acid esters (DBBP) extraction neptunium recovery.Add reductant-oxidant and can introduce impurity and corrosive substance, also can increase the volume of radioactive waste, thereby increase the waste disposal expense.DT-2460145 has proposed a kind of method of separating neptunium in the purex flow process, promptly utilizes the electrolytic reduction method in multi-stage counter current extraction equipment, at the following Pu of low acid
(IV)Electrolytic reduction becomes Pu
(III)The time, N
P (IV)Be reduced into N
P (VI)Thereby, plutonium and neptunium from the TBP organic phase reduction reextraction to water, this moment u
(VI)Still be retained in TBP mutually in, realize that plutonium, neptunium separate the purpose of recovery with uranium.The advantage of this method is not need to increase special extraction cycle, does not change purex flow process condition, can be from purex flow process organic phase neptunium recovery.But there is some weak point in this method, and this method need be built the multi-stage counter current extraction equipment that can carry out electrolytic reduction simultaneously, as electrolysis mixer-settler or electric pulse post.Electrolytic reduction electrode and insulation facility are installed on multi-stage counter current extraction equipment, are made to involve great expense electrolytic reduction mixer-settler or electric pulse rod structure complexity.Because TBP is to N when concentration of nitric acid is higher
P (IV)Certain extracting power is arranged, make the reduction reextraction of neptunium can only be at very low acidity (0.2-1.0mol/l HNO
3) under carry out, and how method does not relate to and coming together into TBP mutually being oxidized to sexavalence with the pentavalent neptunium of sexavalence neptunium coexistence in the purex flow process liquid.
The purpose of this invention is to provide a kind of method of regulating the valence state and the neptunium recovery of neptunium in the high activity liquid waste.This method adopts simple electrolytic reduction equipment, and the method for using electrolytic reduction is reduced into tetravalence to the pentavalent neptunium in the strong radioactive waste liquid in the acidity scope of broad, use the neutral phosphorus extractant that tetravalent neptunium is had very strong extracting power again, as trialkyl (C
6-C
8) phosphine oxide (TRPO) is from aqueous phase extraction tetravalent neptunium, other actinide in the high activity liquid waste comprises that trivalent plutonium and trivalent americium etc. are extracted simultaneously, thereby realizes removing from high activity liquid waste and reclaiming actinide.
Main points of the present invention are to adopt reduction cell, pentavalent neptunium in the radioactive liquid waste is reduced into tetravalence, the structure of electrolytic tank is as follows: negative electrode can adopt tabular titanium negative electrode or platinum electrode, anode can be thread platinum electrode, between the two poles of the earth filter can be set, reference electrode is a mercurous chloride electrode, and electrolysis is carried out under continuous current, and available stirring apparatus stirs electrolytic solution.Add hydrazine in the radioactive liquid waste system of electrolytic reduction, in the system concentration of hydrazine be 0.01mol/l to 0.2mol/l, the temperature of electrolytic reduction is advisable with 20-40 ℃, concentration of nitric acid can be 0.5mol/l to 3.5mol/l in the system.
Main electrode reaction is in this system when electrolysis:
Pentavalent neptunium is reduced on negative electrode:
（1）
Ferric iron is reduced
Following reaction takes place in nitrate radical:
Hydrogen ion is reduced:
The hydrazine ion is oxidized on anode:
In the radioactive liquid waste that the spentnuclear fuel aftertreatment obtains, exist useful elements such as uranium, plutonium, fission product and non radioactive element and corrosion product such as iron etc., they also can produce reaction on electrode, be example with uranium, plutonium, and following reaction takes place on negative electrode:
Nitrous acid (HNO in the negative electrode generation
2) oxidisability is arranged, the N that reduction is obtained
P (IV)Again be oxidized to N
P (V), the adding of hydrazine can destroy nitrous acid and prevent N
P (IV)Reoxidize.
In this system, N
P (V)The electrolytic reduction reacting phase for N
P (V)Concentration follow the first order reaction rate equation, the raising of concentration of nitric acid helps electrolytic reduction, and reaction velocity is accelerated, and also makes that percent reduction increases in the time of determining, table 1 has been listed N
2H
5NO
3-Fe-HNO
3In the system, concentration of nitric acid is to the influence of electrolytic reduction velocity constant.Electrolyte acidity is from 0.5mol/l HNO
3Bring up to 2.5mol/l HNO
3Make the electrolytic reduction rate constant improve nearly 60 times.2 hours percent reduction of electrolytic reduction is brought up to more than 99% from 20%.
Table 1 pH is to N
P (V)The influence of electrolytic reduction velocity constant
(N
P (V))
Initially=4mg/l (Fe
(III))
Initially=2g/l
(N
2H
5NO
3)
Initially=0.2mol/l
Current density: 29mA/cm
2Temperature: 30 ℃
| HNO 3mol/l | 0.50 | 0.75 | 1.00 | 1.50 | 2.50 |
| K×10 2min －1 | 0.152 | 0.379 | 1.27 | 3.42 | 8.90 |
The existence of hydrazine in the system can destroy nitrous acid, prevents N
P (IV)Reoxidize.The concentration of hydrazine is to N
P (V)The reduction rate influence is little.When hydrazine concentration rate constant when 0.01mol/l is increased to 0.2mol/l only doubles.When hydrazine concentration is too high, can form the intermediate product hydrazoic acid in system, it is a kind of explosive material, so the concentration of hydrazine is difficult too high, can not surpass 0.2mol/l.Ferric ion is to N in the system
P (V)Electrolytic reduction played facilitation.There is not under the ferric ion situation N
P (V)Electrolytic reduction speed very slow, Fe
(III)Under the existence of ion (as 2g/l), N
P (V)The electrolytic reduction velocity constant improve tens times.Iron is that the reductive agent of tetravalence plutonium also is a corrosion product in the purex flow process, has ferric ion in the high activity liquid waste that the spentnuclear fuel aftertreatment obtains usually, needn't add in addition.
Temperature improves, and help improving reduction rate and improve percent reduction, but the too high meeting of temperature causes solution evaporation, complicated operation, operating temperature should not be higher than 50 ℃, is advisable with 20-40 ℃.
N in the system
2H
5NO
3With by N
2H
5NO
3The Fe of reduction
(II)Itself also can be N
P (V)Be reduced into N
P (IV), but reduction rate is slower, and the percent reduction in the certain hour is lower.Under the condition of electrolytic reduction, N
P (V)Reduction rate accelerate greatly, the percent reduction in the certain hour also improves greatly.
In the high activity liquid waste system that the spentnuclear fuel aftertreatment obtains, N
P (V)Reduction ratio N
2H
5NO
3-Fe-HNO
3More favourable in the system.In the analog material liquid of preparation, N
P (V)Electrolytic reduction quicken concentration of nitric acid greatly and increase N
P (V)Electrolytic reduction influence more obvious.Table 2 has been listed the composition of simulated high-level radioactive waste, and table 3 has been listed concentration of nitric acid to N in the analog material liquid
P (V)The influence of electrolytic reduction.
The composition of table 2 simulated high-level radioactive waste (continued)
| Element | Nd | Ce | Na | Fe | Zr |
| Concentration mol/l | 0.0243 | 0.0143 | 0.235 | 0.036 | 0.022 |
The composition of table 2 simulated high-level radioactive waste (having continued)
| Element | Mo | Ru | u | HNO 3 |
| Concentration mol/l | 0.019 | 0.003 | 0.002 | On demand |
Concentration of nitric acid is to N in table 3 analog material liquid
P (V)The influence of reduction
Add (N
2H
5NO
3)
Just=0.2mol/l, temperature: 30 ℃
In simulated high-level radioactive waste, uranium is become tetravalence by electrolytic reduction.Because the effect of multivalent ions such as uranous catalytic action and ruthenium molybdenum makes N
P (V)Reduction rate improve greatly.When analog material liquid acidity is 1.5mol/l HNO
3The time, in the presence of the 0.2mol/l hydrazine, through electrolytic reduction in half an hour, whole N almost
P (V)Be reduced into N
P (IV)Improving the concentration of nitric acid reduction rate also can improve.
At N
P (V)In the time of by electrolytic reduction, the tetravalence plutonium in the high activity liquid waste is reduced into Pu
(III), a spot of uranyl ion is reduced into uranous.
Neutral phosphorus extractant mixed trialkylphosphinyl R
3PO(is R=C wherein
6～C
8Potpourri), actinide is had very strong extracting power (Chinese patent application number 85105352).In table 4, listed 2.0 and 4.0mol/l HNO
3Following 30%(volume) TRPO-kerosene is to the extraction of uranium, plutonium, neptunium, americium.Therefore high activity liquid waste is carried out N
P (V)Electrolytic reduction after, use the 30%(volume) TRPO-kerosene is through the extraction of 1-2 level, can remove uranium, plutonium, neptunium, perhaps (≤2mol/l HNO under medium acidity
3) strong radioactive waste liquid is at N
P (V)Behind the electrolytic reduction, use the 30%(volume) what counter-current extraction of TRPO-kerosene process, can remove and reclaim all actinides.Collection is gone into the americium curium of organic phase can use 3.5-5mol/l HNO
3Back extraction, neptunium, plutonium be with 5% oxalic acid back extraction, and uranium is with 5% sodium carbonate back extraction.
The present invention has overcome electrolytic reduction device structure complexity, and the shortcoming that cost is high requires the low restriction of acidity when also having overcome electrolytic reduction, does not introduce corrosion and foreign ion except a small amount of hydrazine in system, does not increase the radioactive waste volume.It is simple to have the electrolytic reduction device structure, cost is low, the percent reduction height of neptunium, the advantage that can remove whole actinides in the high activity liquid waste under appropriate condition simultaneously is specially adapted to removal and recovery that the aftertreatment of reactor spentnuclear fuel obtains actinide in the high activity liquid waste.
Table 4 30%(volume) TRPO-kerosene is to the extraction (trace quantity) of actinide
| HNO 3 | Am 3+ | Pu 3+ | Pu 4+ | Np 4+ | uo 2 2+ |
| 2mol/l | 1.8 | 29 〔1〕 | ＞1000 〔1〕 | ＞100 | ＞1000 〔1〕 |
| 4mol/l | 0.15 | － | ＞1000 〔1〕 | ～400 〔1〕 | ＞1000 〔1〕 |
Annotate: (1) data are from nuclear chemistry and radiochemistry 7(2 such as Jiao Rongzhou) 65(1985) estimated value of middle Fig. 1
Embodiment one
The electrolytic reduction device as shown in Figure 1, wherein 1 is electrolytic cell, 2 is calibration cell, 3 is the titanium negative electrode, 4 is platinum anode, and 5 is calomel reference electrode, and 6 is salt bridge, and 7 is saturated potassium chloride solution, 8 is potentiostat, and 9 is digital voltmeter, and 10 is milliammeter, and 11 are temperature control meter.Electrolytic cell is cylindrical, and diameter is 40mm, and electrode separation is 30mm, and anode is the platinum filament coiled, and area is 1.57cm
2Negative electrode is the titanium plate, and area is 1.38cm
2There is not filter between the electrode.Electrolytic solution 40ml, it consists of: N
2H
5NO
3, 0.2mol/l; Fe
(III), 2g/l; HNO
3, 2.5mol/l, N
P (V)Solution is preparation newly before experiment, adds when electrolysis begins, and its concentration is about 5mg/l.Electrolysis is carried out under 30 ℃, and current density is 29mA/cm
2, superpressure is the 1.5-2 volt, cathode potential is about the fluctuation of 0.7-0.9 volt.The electrolytic cell electromagnetic agitation, after electrolysis in 2 hours, neptunium is reduced into tetravalence, uses the 30%(volume) the TRPO-kerosin, compare organic phase/water=1,99% neptunium is reclaimed in the one-level extraction.
Embodiment two
The electrolytic reduction device as shown in Figure 1, electrolyser construction such as example one.Electrolytic solution 40ml is simulated high-level radioactive waste, and it is formed as table 2, concentration of nitric acid＞2mol/l.Neptunium is with pentavalent N
PO
+
2Form adds, and adding hydrazine when electrolysis begins, to make its concentration be 0.2mol/l.Electrolysis is carried out under 30 ℃, and current density is 29mA/cm
2, use electromagnetic agitation electrolytic solution.99.9% neptunium is reduced into tetravalence behind 30 minutes electrolytic reductions, and plutonium is reduced into trivalent.Use the 30%(volume) the TRPO-kerosin, to compare organic phase/water=1,＞99% uranium, plutonium, neptunium are reclaimed in the secondary extraction.
Embodiment three
The electrolytic reduction device as shown in Figure 1, electrolyser construction such as example one.Electrolytic solution is the simulated high-level radioactive waste through the part denitration, and it is formed as table 2, concentration of nitric acid＜2mol/l, and as 1.5mol/l, the electrolytic reducting liquid volume is 40ml.Neptunium is with pentavalent N
PO
+
2Form adds, and adds hydrazine when electrolytic reduction begins, and its concentration is 0.2mol/l.Temperature is 30 ℃, and current density is 29mA/cm
2Be reduced into tetravalence through 30 minutes electrolytic reduction 99.9% neptuniums, meanwhile plutonium is reduced into trivalent.Use the 30%(volume) the TRPO-kerosin, with the stream ratio of organic phase/water=1, the extraction of six stage countercurrents can be removed and reclaim＞99% uranium plutonium, neptunium and americium.Water becomes the high activity liquid waste that does not contain αHe Su.
Claims (1)
- The method of a kind of electrolytic reduction-extraction neptunium recovery from acid radioactive liquid waste extracts neptunium recovery after adopting electrolytic reduction that the pentavalent neptunium in the waste liquid is reduced to tetravalent neptunium, it is characterized in that:1, said electrolytic reduction is to carry out in electrolytic tank, and the structure of electrolytic tank is that negative electrode can adopt tabular titanium plate or platinum electrode, and anode can be thread platinum electrode, between the two poles of the earth filter can be set, and reference electrode is a mercurous chloride electrode.2, add hydrazine in the said acid radioactive liquid waste system, the concentration of hydrazine is 0.01mol/l-0.2mol/l in the system.3, the temperature of electrolytic reduction is advisable with 20-40 ℃.4, the concentration of nitric acid of said acid radioactive liquid waste system is 0.5mol/l-3.5mol/l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88104195 CN1012771B (en) | 1988-07-14 | 1988-07-14 | Electrolytic reduction-extraction method for reclaiming np from waste radio active liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88104195 CN1012771B (en) | 1988-07-14 | 1988-07-14 | Electrolytic reduction-extraction method for reclaiming np from waste radio active liquor |
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| Publication Number | Publication Date |
|---|---|
| CN1039321A true CN1039321A (en) | 1990-01-31 |
| CN1012771B CN1012771B (en) | 1991-06-05 |
Family
ID=4832919
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88104195 Expired CN1012771B (en) | 1988-07-14 | 1988-07-14 | Electrolytic reduction-extraction method for reclaiming np from waste radio active liquor |
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1988
- 1988-07-14 CN CN 88104195 patent/CN1012771B/en not_active Expired
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|---|---|
| CN1012771B (en) | 1991-06-05 |
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